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CHM 260





: 2013219228


: AS1206A2




: 8th JANUARY 2016

1.0 AIM
To identify the qualitative analysis of an unknown benzoic acid using Fourier Transform
Infrared Spectrometers (FTIR).

FTIR spectrometry is used for the identification of chemical and pharmaceutical
substances. In the recent past the use of FTIR spectroscopy with appropriate software has
been used for solving different problems related to analytical development. In addition, this
technique is also known for its low cost, simplicity, non- destructiveness and rapidity for
qualitative analysis.
FTIR (Fourier Transform Infrared) spectrometry was developed in order to overcome the
limitations encountered with dispersive instruments. The main difficulty of this method is the
scanning process was too slowed. To counter this problem, a solution was developed which
employed a very simple optical device called as interferometer. This solution produces a
unique type of signal which has all of the infrared frequencies encoded into it. As a result,
the signal can be measured very quickly, usually on the order of one second or so. Thus, the
time element per sample is reduced to a matter of a few seconds rather than several minutes.
Most interferometers employ a beam splitter which takes the incoming infrared beam and
divides it into two optical beams. One beam reflects off of a flat mirror which is fixed in
place. The other beam reflects off of a flat mirror which is on a mechanism which allows this
mirror to move a very short distance (typically a few millimetres) away from the beam
splitter. The two beams reflect off their respective mirrors and are recombined when they
meet back at the beam splitter. The path that one beam travels is a fixed length and the other
is constantly changing as its mirror moves, the signal which exits the interferometer is the
result of these two beams interfering with each other. The resulting signal is called an
interferogram which has the unique property that every data point which makes up the signal
has information about every infrared frequency which comes from the source.

Figure 1: Schematic diagram of FTIR

Benzoic acid is a solid that is crystalline in appearance, similar to white needles. A natural
source of benzoic acid is gum benzoin, which comes from certain tree barks; however,
benzoic acid can also be made by synthetic means. The substance received its name from
gum benzoin, the plant from whose resin it was first derived (Joseph, 2013). The chemical
formula of benzoic acid is C7H6O2: it has seven carbon (C) atoms, six hydrogen (H) atoms
and two oxygen (O) atoms. This chemical formula can also be written as C6H5COOH. The
chemical structure of carboxylic acid is shown below. On the left, it shows all the carbon and
hydrogen atoms on the benzene ring, and on the right, it shows another way to draw the
benzene ring, which is drawn in blue. Benzoic acid is an organic compound because it
contains carbon, and it is also an aromatic carboxylic acid. It is aromatic because it has a
benzene ring in its chemical structure (the hexagon with double bonds illustrated in blue),
where the benzene ring has alternating double bonds between each carbon. It is classified as a
carboxylic acid because it has a carboxyl group in its structure, which is the COOH group.

Figure 2: Chemical Structure of Benzoic Acid


Benzoic acid occurs naturally in various berries notably cranberries, cinnamon,
plums, currants, cloves, etc. It has long been used to inhibit microbial growth in many
products including non-alcoholic beverages, jams and emulsified sauces. The salt of
benzoate is more stable than the acid form and more soluble in water making the
benzoate a favourable choice for the soft drinks industry. In addition, benzoic acid
was used as a major preservative compound in fermented fish products such as
cencaluk, budu and dried fish (Norlida, 2009).
Norlida (2009) also state that this compound are effective to prevent the growth of
yeast, mould and a wide range of bacteria, proving that benzoic acid is an important
compound in economic industrial such as food production.

3.2 FT-IR
Fourier Transform Infrared Spectrometers (FTIR) is a technique that used to obtain
an infrared spectrum or emission of a solid, liquid or gas. An FTIR spectrometer
simultaneously collects high spectral resolution data over a wide spectra range. This
converse a significant advantage over a dispersive spectrometer which measures
intensity over a narrow range of wavelengths at a time.
In infrared spectroscopy, an infrared (IR) radiation is passed through the sample.
Some of the infrared radiation is absorbed by the sample and some of it passed
through (transmitted). As a result, the spectrum represents the spectrum represents the
molecular absorption and transmission, creating a molecular fingerprint of a sample.
FTIR are widely used by the researchers as a method to complete their studies.
According to Kappler (2015), FTIR has been used analyze the samples of
microplastics in aquatic ecosystems qualitatively and quantitatively by collecting the
information and make an appropriate and reliable analytical methods to distinctly
identify and also to quantify these particles in environmental sample.
On the other hand, FTIR is also play an important role in a medical field. Nuria
(2014) states that FTIR has been used to co-localize amyloid deposits and lipid
peroxidation in tissue slides from patients that affected by Alzheimers disease.

To prepare the KBr pellet of benzoic acid
To carry out a qualitative analysis of benzoic acid using FT-IR

To identify IR absorption peaks and the corresponding functional groups of an

unknown solid/liquid/powder.


There are several important chemical and instrument to conduct this experiment such
as benzoic acid, potassium bromide (KBr), KBr pallet apparatus (die, hydraulic press,
grinder, etc) and FTIR instrument.

6.1 The KBr Method
The solid sample (benzoic acid) and the KBr solid (IR grade) will be obtained
from the desiccator. Each of samples will be weighed about 1 gram and dry in
the oven for about 2-3 hours at 110C. (This step may be done ahead of time
with help of the laboratory staff). Next, the agate mortar and pestle will be
removed from the desiccator for use to grind the benzoic acid and KBr. After
that, about 1 mg of benzoic acid will be taken and grinding by using agate
mortar for about 1 minute or more and pestle until the benzoic acid become
very small and shiny. Hence, about 80 mg of KBr will be take and grinded by
using agate mortar and pestle until it becomes powdered. The benzoic acid and
powdered KBr will be mixed in agate mortar for ratio 1:80 and grind the
mixture until become homogeneous for about 30 seconds. Using the spatula,
the mixture will be scraped into the middle and the mixture will be grinded
again about 15 seconds to mix the benzoic acid thoroughly with the KBr. The
benzoic acid and KBr must be finely ground, or the mixture will scatter the
infrared radiation excessively. The mixture will be heaped in the center of the
agate mortar using a spatula.

6.2 Making the KBr Pellet

The die set will be removed from the box or storage container. Then, the die
set will be cleaned with Ethanol. The mixture of benzoic acid and KBr will be
put into the die set and make sure the mixture fills the surface of the die set.
Next, the die set will be tighten closely and placed into hydraulic press gauge.

The Hydraulic Press gauge will be press until the pressure goes up to 7000 psi.
Release the air and let it rest for 2 minutes. The Hydraulic Press gauge will be
pressed again until the pressure goes up to 8500 psi and will be rested for 1
minute. Release the pressure. The die set will be remove slowly from the
Hydraulic Press gauge. After that, the die set and the KBr pellet will be
opened. The compound that obtained should appear clear like a piece of glass
or transparent disk. Lastly, the KBr pellet will be placed into a pellet holder for
6.3 Preparing Liquid Samples (neat liquids) using a Salt Plate
Firstly, a neat liquid sample will be used. Then, some of the liquid sample
will be placed about 12 drops on the plate and covered with another plate. The
liquid should be spread out to cover the entire plate. After that, the sandwich
will be place in the IR salt plate holder and will be covered with a hold-down
plate. Next, at least 2 nuts will be placed on the posts of the holder and the
nuts will be rotated gently to hold the plates with an even pressure. Do not
force it because it will be cracking the plates. Next, the holder will be slide
into the bracket on the instrument in the sample beam and the spectrum will be
conducted. Lastly, the salt plates will be removed and cleaned from the
instrument. Often a little acetone followed by drying with Kim Wipes will do.
The salt plates will be kept in a clean and dry place.

6.4 Sample preparation for FT-IR (Reflectance)

The solid samples will be grounded finely before use. Next, the spectrum of
benzoic acid will be conducted using the Reflectance method. Lastly, an
unknown will be obtained from the lab instructor and the spectrum will be

Figure 3: Infrared Spectra of Benzoic Acid

Wavenumber (cm-1)

Type of bond

Functional Group
Carboxylic acid

Table 1: Tabulation Data of Infrared Spectra of Benzoic Acid


FTIR is preferred over dispersive or filter methods of infrared spectral analysis. This
is because this method has many advantages. Speed is one of the main reasons. All of
the frequencies that are measured, most measurements by FTIR are made in a few
seconds. Other than that, it provides excellent sensitivity. The detectors are much
more sensitive, the optical throughput is much higher. FTIR also internally calibrated,
this instruments use a HeNe laser as an internal wavelength calibration standard. This
HeNe laser are self-calibrating. These advantages make measurements made by FT-IR
extremely accurate. Thus, it is a reliable technique for positive identification of

virtually any sample. The sensitivity benefits enable identification of even the
smallest of contaminants. This makes FT-IR a very good tool for quality control.

Joseph, K., & Kingsley, B (2013). Solubility of Benzoic Acid in Pure Solvents and
Binary Mixtures. Journal of Chemical & Engineering Data, 55(11), 7-13
Norlida, B., (2009). Determination of Benzoic Acid in Fermented Fish Products using
HPLC. QD Chemistry, 16(7), 176
Kappler, A., Windrich, F., Frank, L., Malanin, M., & Klaus-Jochen, V. (2015).
Identification of Microplastics by FTIR and Raman Microscopy. Analytical and
Bioanalytical Chemistry, 407(22), 6791
Benseny-Cases, N., Nuria, K., Oxana, C., Marine, F., & Cladera, J. (2014). Analytical
Chemistry. American Chemical Society, 86(24), 1204-12